Method for preventing an unauthorized use of disposable bioprocess components

ABSTRACT

This invention provides a system and apparatus that is able to authenticate and prevent illegal manufacturing and unauthorized operation of disposable bioprocess components. This invention utilizes a ferro-electric random access memory chip (FRAM) chip to store error-correctable information on a RFID tag attached to the disposable bioprocess components, where the error-correctable information is written in sequence into the memory chip, so that the redundant information can remain in the chip when the RFID tag and disposable bioprocess component is gamma-sterilized. Also, this invention includes a method for authenticating the disposable bioprocess component that reduces liability in that a counterfeit poor quality disposable component is not used on the hardware so the user will not file an unjustified complaint.

CROSS-REFERENCE TO RELATED APPLICATIONS

This application is a filing under 35 U.S.C. §371 and claims priority tointernational patent application number PCT/US2008/073625 filed Aug. 20,2008, published on Oct. 1, 2009, as WO 2009/120232, which claimspriority to U.S. provisional patent application No. 61/039,964 filed onMar. 27, 2008; the disclosure of which is incorporated herein byreference in its entirety.

FIELD OF THE INVENTION

This invention relates to a radio frequency identification system thatdetects illegal manufacturing and prevents unauthorized operation ofdisposable bioprocess components

BACKGROUND OF THE INVENTION

Radio frequency identification (RFID) tags are widely employed forautomatic identification of objects, such as animals, garments etc. anddetection of unauthorized opening of containers. There are severalexamples of RFID tags being used to identify objects.

First, there is a U.S. Pat. No. 7,195,149 for a method of attaching anRFID tag to a hose and tracking system. This hose tracking systemincludes a hose assembly with an attached RFID tag embedded thereinduring manufacture, molded thereon permanently attached. The RFID tag iscoded with an identification specific to the particular hose assembly.An RFID tag reader is provided, which is usable by a user to obtain theidentification from the RFID tag on the hose, preferably after it isinstalled at the user facility. The RFID tag reader includes a userinput for at least one trackable event and is at least connectable to acomputer network or compatible for uploading the identification and anyuser input to a network accessible device. A network accessible hosedatabase is provided, having hose-related information. The networkaccessible hose database provides access to a user to obtain thehose-related information based on the identification from the RFID tagthat receives and stores data related to the at least one trackableevent. There is also another U.S. Pat. No. 7,328,837 similar to U.S.Pat. No. 7,195,149, where U.S. Pat. No. 7,328,837 is for a method ofattaching an RFID tag to a hose and tracking system.

Next, there is U.S. Pat. No. 5,892,458 that is an apparatus for therecognition of exchangeable parts in analytical measuring instruments.The apparatus for the recognition of exchangeable parts in an analyticalmeasuring instrument or in an analytical measurement system with severalanalytical devices contain exchangeable parts that have identificationmodules that are each attached to an exchangeable part. In addition, theapparatus has transmitter receiver devices that can receive informationsignals from an identification module and send information signals tothe identification module. The control device can cause a message to bedisplayed on a display device if the information read out from anidentification module does not fulfill certain conditions, for examplewith regard to the quality.

Next, there is another U.S. Pat. No. 7,135,977 for a method and systemfor tracking identification devices, which includes storing data aboutthe identification device in a register, the data to be stored includingdata relating to a forwarding location that requests information aboutthe identification device should be forwarded. The identification deviceis attached to an item to be monitored. The method includes accessingthe register when the identification device has been read and a requestfor information has been received. Details of the forwarding locationare obtained from the register. The request is forwarded to theforwarding location and the requested information about theidentification device is sent from the forwarding location to arequester of the information.

While the aforementioned RFID inventions have been able to identifydevices associated with the RFID tags, these inventions are not able toauthenticate and prevent illegal manufacturing and unauthorizedoperation of gamma sterilizable disposable bioprocess components.Therefore, there is a need for an apparatus and system that is able toauthenticate and prevent illegal manufacturing of disposable bioprocesscomponents, especially those that are sterilized by gamma irradiation orother suitable means of lowering bio-burden of the disposable or limitedreuse device.

BRIEF SUMMARY OF THE INVENTION

The present invention has been accomplished in view of theabove-mentioned technical background, and it is an object of the presentinvention to provide a system and method for authenticating disposablebioprocess components attached to RFID tags.

In a preferred embodiment of the invention, there is a method forpreventing an unauthorized use of a disposable bioprocess component. Themethod includes: fabricating an RFID tag and a disposable component;integrating the RFID tag with the disposable component; initializing thememory chip by applying RF signal to the complementary metal-oxidesemiconductor (CMOS) circuitry; writing error-correctable information toa ferroelectric random memory (FRAM) portion part of a memory chip ofthe RFID tag; sterilizing the disposable component with the integratedRFID tag; assembling the disposable component in a biological fluidflow; detecting and correcting possible errors in written data caused bygamma irradiation; and determining if the disposable bioprocesscomponent is authenticated.

In another preferred embodiment of the invention, there is a method forpreventing an unauthorized use of a disposable bioprocess component. Themethod includes: fabricating an RFID tag and a disposable component;integrating the RFID tag with the disposable component; initializing thememory chip by applying RF signal to the complementary metal-oxidesemiconductor (CMOS) circuitry and writing error-correctable informationto a plurality of regions on a ferroelectric random memory (FRAM)portion part of a memory chip of the RFID tag; sterilizing thedisposable component with the integrated RFID tag; assembling thedisposable component in a biological fluid flow; and determining if thedisposable bioprocess component is authenticated.

In yet another preferred embodiment of the invention, there is a methodfor preventing an unauthenticated use of a disposable bioprocesscomponent. The method includes: integrating an RFID tag with adisposable component; writing error-correctable information on aFerro-electric random access memory (FRAM) chip of the RFID tag;sterilizing the disposable bioprocess component with the integrated RFIDtag; assembling the disposable component in a biological fluid flow;determining the information on the RFID tag in the disposable bioprocesscomponent; determining if the disposable bioprocess component isauthenticated; and releasing digital data on the RFID tag if theinformation on the RFID tag in the disposable bioprocess component isauthenticated.

In another preferred embodiment of the invention, there is a method forpreventing an unauthorized use of a disposable bioprocess component withthe RFID tag where the memory of the memory chip of the tag has amaximum available data capacity. The method includes: fabricating anRFID tag that includes a memory chip that contains both a CMOS circuitryand a FRAM circuitry; fabricating a disposable bioprocess component;integrating the RFID tag with the disposable bioprocess component;initializing the memory chip by applying RF signal to the CMOS circuitryand writing redundant information to a plurality of regions in the FRAMcircuitry of the memory chip of the RFID tag; sterilizing the disposablebioprocess component with the integrated RFID tag; assembling thedisposable bioprocess component in a biological fluid flow;authenticating the disposable bioprocess component with the RFID tag;and releasing the available memory from the redundant memory blocks tothe end-user.

In another embodiment of the invention, there is a method for preventingan unauthorized use of a disposable bioprocess component with an RFIDtag where the memory chip of the tag has the radiation-hardened CMOSstructure of the memory chip and a non-volatile memory. The methodincludes: fabricating an RFID tag with a memory chip that contains botha radiation-hardened CMOS circuitry and a FRAM circuitry, fabricating adisposable bioprocess component; integrating the RFID tag with thedisposable bioprocess component; initializing the memory chip byapplying RF signal to the radiation-hardened CMOS circuitry and writingredundant information to a plurality of regions in FRAM part of thememory chip of the RFID tag; sterilizing the disposable bioprocesscomponent with the integrated RFID tag; assembling the disposablebioprocess component in a biological fluid flow vessel or purificationcomponent; and authenticating the disposable bioprocess component withthe RFID tag.

In another embodiment of the invention, there is a method for preventingan unauthorized use of a disposable bioprocess component with an RFIDtag that contains both a CMOS circuitry and a FRAM circuitry. The methodincludes: fabricating an RFID tag with a memory chip that contains botha CMOS circuitry and a FRAM circuitry, fabricating a disposablebioprocess component; integrating the RFID tag with the disposablebioprocess component; initializing the memory chip by applying RF signalto the CMOS circuitry and writing redundant information to a pluralityof regions in FRAM part of the memory chip of the RFID tag;gamma-sterilizing the disposable bioprocess component with theintegrated RFID tag; assembling the disposable bioprocess component in abiological fluid flow; recovering the CMOS circuitry after the gammairradiation, and authenticating the disposable bioprocess component withthe RFID tag.

In yet another embodiment of the invention, there is a method forpreventing an unauthorized use of a disposable bioprocess component withan RFID tag that has a memory chip that contains both a CMOS circuitryand a FRAM circuitry of the RFID memory chip. The method includes:fabricating an RFID tag that includes a memory chip that contains both aCMOS circuitry and a FRAM circuitry, fabricating a disposable bioprocesscomponent; integrating the RFID tag with the disposable bioprocesscomponent; initializing the memory chip by applying RF signal to theCMOS circuitry and writing redundant information to a plurality ofregions in FRAM part of the memory chip of the RFID tag, where writingof redundant information to a plurality of regions in FRAM part of thememory chip of the RFID tag is accomplished by sending information onlyonce to the RFID tag and sending the number of desired redundancy; andthe memory chip configured to write redundant information into memoryblocks; sterilizing the disposable bioprocess component with theintegrated RFID tag; assembling the disposable bioprocess component in abiological fluid flow; reading of redundant information from a pluralityof regions in FRAM part of the memory chip of the RFID tag, wherereading is done from the redundant memory blocks and comparing theinformation from redundant blocks, and releasing only the most redundantinformation; and authenticating the disposable bioprocess component withthe RFID tag.

In yet another embodiment of the invention, there is a method forpreventing an unauthorized use of a disposable bioprocess component. Themethod includes: fabricating an RFID tag that includes a memory chipthat contains both a CMOS circuitry and a FRAM circuitry, fabricating adisposable bioprocess component; integrating the RFID tag with thedisposable bioprocess component; initializing the memory chip byapplying RF signal to the CMOS circuitry and writing error-correctableinformation to FRAM part of the memory chip of the RFID tag, encryptingthe information; sterilizing the disposable bioprocess component withthe integrated RFID tag; assembling the disposable bioprocess componentin a biological fluid flow; decrypting information; and authenticatingthe disposable bioprocess component with the RFID tag.

In another embodiment of the invention, there is a method for preventingan unauthorized use of a disposable bioprocess component. The methodincludes: fabricating an RFID tag that includes a memory chip thatcontains both a CMOS circuitry and a FRAM circuitry, fabricating adisposable bioprocess component; adapting the RFID tag for physical,chemical, or biological sensing in disposable bioprocess component;integrating the resulting RFID sensor with the disposable bioprocesscomponent; initializing the memory chip by applying RF signal to theCMOS circuitry and writing error-correctable information to FRAM part ofthe memory chip of the RFID sensor where information containscalibration parameters of the RFID sensor; sterilizing the disposablebioprocess component and the integrated RFID sensor; assembling thedisposable bioprocess component in a biological fluid flow; andauthenticating the disposable bioprocess component and the RFID sensor.

In another embodiment of the invention, there is a method for preventingan unauthorized use of a disposable bioprocess component. The methodincludes: fabricating an RFID tag that includes a memory chip thatcontains a CMOS circuitry, a FRAM circuitry, and analog input from aphysical, chemical, or biological sensor, attaching at least onephysical, chemical, or biological sensor to the memory chip, fabricatinga disposable bioprocess component; integrating the resulting RFID sensorwith the disposable bioprocess component; initializing the memory chipby applying RF signal to the CMOS circuitry and writingerror-correctable information to a plurality of regions in the FRAMcircuitry of the memory chip of the RFID sensor where theerror-correctable information contains calibration parameters of theRFID sensor; sterilizing the disposable bioprocess component and theintegrated RFID sensor; assembling the disposable bioprocess componentin a biological fluid flow; and authenticating the disposable bioprocesscomponent with the RFID sensor where authentication involves RFID sensorinitialization and a change of its reading.

In another embodiment of the invention, there is a method for preventingan unauthorized use of a disposable bioprocess component with an RFIDtag that contains both a CMOS circuitry and a FRAM circuitry. The methodincludes: fabricating an RFID tag with a memory chip that contains botha CMOS circuitry and a FRAM circuitry, fabricating a disposablebioprocess component; integrating the RFID tag with the disposablebioprocess component; initializing the memory chip by applying RF signalto the CMOS circuitry and writing error-correctable information to FRAMpart of the memory chip of the RFID tag; gamma-sterilizing thedisposable bioprocess component with the integrated RFID tag; assemblingthe disposable bioprocess component in a biological fluid flow, andauthenticating the disposable bioprocess component with the RFID tagwhen RFID tag reading is performed at different power levels of the RFIDtag reader or at different distances between the reader and the RFIDtag.

BRIEF DESCRIPTION OF THE DRAWINGS

These and other advantages of the present invention will become moreapparent as the following description is read in conjunction with theaccompanying drawings, wherein:

FIG. 1 illustrates a block diagram of a system in accordance with anembodiment of the invention;

FIG. 2 shows a radio frequency identification (RFID) tag of FIG. 1 inaccordance with an embodiment of the invention;

FIG. 3 illustrates a schematic of a memory chip of the RFID tag of FIG.1 in accordance with an embodiment of the invention;

FIGS. 4A and 4B depict a block diagram of redundant information storedin the RFID chip of FIG. 2 in accordance with an embodiment of theinvention;

FIG. 5 depicts a flow-chart of the operation of a disposable componentwith the (RFID) tag of FIG. 1 in accordance with an embodiment of theinvention;

FIG. 6 illustrates the memory chip of FIG. 3 divided into sectors inaccordance with an embodiment of the invention;

FIG. 7 shows a schematic of an operation of the memory chip of FIG. 3 inaccordance with the invention; and

FIG. 8 illustrates a table of how the RFID tag operates in accordancewith an embodiment of the invention.

DETAILED DESCRIPTION OF THE INVENTION

The presently preferred embodiments of the invention are described withreference to the drawings, where like components are identified with thesame numerals. The descriptions of the preferred embodiments areexemplary and are not intended to limit the scope of the invention.

FIG. 1 illustrates a block diagram of a system for measuring parametersin a container. The system 100 includes a container 101, a radiofrequency identification (RFID) tag 102, a standard computer 109 and ameasurement device (writer/reader) 111, which includes a reader 106. Thetag 102 is incorporated or integrated into the container 101. RFID tag102 may also be referred to as tag 102.

Container 101 may be a disposable bio-processing container, a cellculture bioreactor, a mixing bag, a sterilization container, a metalcontainer, a plastic container, a polymeric material container, achromatography device, a filtration device, a chromatography device withany associated transfer conduits, a filtration device with anyassociated transfer conduits, centrifuge device, a connector, a fitting,a centrifuge device with any associated transfer conduits, apre-sterilized polymeric material container or any type of containerknown to those of ordinary skill in the art. In one embodiment, thebiological container 101 is preferably made from but not limited to thefollowing materials, alone or in any combination as a multi-layer film:ethylene vinyl acetate (EVA) low or very low-density polyethylene (LDPEor VLDPE) ethyl-vinyl-alcohol (EVOH) polypropylene (PP), polyethylene,low-density polyethylene, ultra-low density polyethylene, polyester,polyamid, polycarbontate, fluoropolymers such as Fluorinated ethylenepropylene (FEP) (made by E. I. du Pont de Nemours and Company located inWilmington, Del.) and Polyvinylidene Fluoride (PVDF), elastomericmaterials all of which are well known in the art. A RFID tag typicallycomprise for an antenna and a microchip with a plastic backing (e.g.,polyester, polyimide etc).

Also, the container 101 may be made of a multilayer bio-processing film,made from one manufacturer. For example, the manufacturer may be GEHealthcare, located in Somerset, N.J., Piscataway, N.J., Westborough,Mass., Newport or Millipore in CA or MA, or Hyclone located in Logan,Utah, for example HyQ® CX5-14 film and HYQ® CX3-9 film. The CX5-14 filmis a 5-layer, 14 mil cast film. The outer layer of this film is made ofa polyester elastomer coextruded with an EVOH barrier layer and anultra-low density polyethylene product contact layer. The CX3-9 film isa 3-layer, 9 mil cast film. The outer layer of this film is a polyesterelastomer coextruded with an ultra-low density polyethylene productcontact layer. The aforementioned films may be further converted intodisposable bio-processing components in a variety of geometries andconfigurations all of which can hold a solution 101 a. In yet anotherembodiment of the invention, the container 101 may be a polymer materialincorporated into a filtration device. Further, the container 101 mayinclude or contain a chromatographic matrix.

Depending on the material of the container, the RFID tag 102 isconnected by a wireless connection to the measurement device(writer/reader) 111 and the computer 109. Container 101 may also be avessel that contains a fluid such as liquid or gas, where the vessel canhave an input and an output. Further, container 101 can have a liquidflow or no liquid flow. Furthermore, container 101 can be a bag, a tube,or a pipe, or a hose.

FIG. 2 is the RFID tag 102. RFID tag 102 is gamma radiation resistant totypical levels required for pharmaceutical processing (25 to 50 kGy).The gamma radiation resistance (immunity to effects of gamma radiation)is provided in several ways: 1. from the storage of required digitalinformation that allows its error correction; 2. from the use ofradiation-hardened CMOS circuitry on RFID tag or from control ofrecovery of the standard CMOS after gamma irradiation; 3. from the useof FRAM memory; and 4. from the reading of the RFID tag after gammaradiation with different power levels of the reader or at differentdistances between the reader and the RFID tag. The first component ofthe RFID tag 102 is an integrated circuit memory chip 201 for storingand processing information and modulating and demodulating a radiofrequency signal. Also, memory chip 201 can also be used for otherspecialized functions, for example it may contain a capacitor. It mayalso contain an input for an analog signal. A second component for thisRFID tag 102 is an antenna 203 for receiving and transmitting the radiofrequency signal.

Storage of required digital information that allows the error correctionof this information is done by using known methods. Non-limitingexamples of these methods include redundancy, Reed-Solomon errorcorrection (or code), Hamming error correction (or code), BCH errorcorrection (or code), and others known in the art.

Data redundancy is achieved by writing multiple copies of the data intomemory so as to protect them from memory faults. Writing multiple copiesof the data into the memory or writing redundant information on a FRAMchip 201 b (FIG. 3) of the RFID tag 102 means writing information intoplurality of regions on the memory chip. The goal of writing redundantinformation on a FRAM chip of the RFID tag is to reduce gammairradiation effect that otherwise can cause loss of at least portion ofdata that will lead to the failure to authenticate a disposablebioprocess component attached to the RFID tag.

The Reed-Solomon error correction is the method used for detecting andcorrecting errors as described in U.S. Pat. Nos. 4,792,953 and4,852,099. This error correction method was used for example, in compactdisks and digital video disks. In order to detect and correct errors indata from RFID tags, the data to be written is converted intoReed-Solomon codes by a computer algorithm and the codes are written tothe RFID memory. When the codes are read back from the RFID memory, theyare processed through a computer algorithm that detects errors, uses theinformation within the codes to correct the errors, and reconstructs theoriginal data.

The Hamming error correction has been used in random access memory(RAM), programmable read-only-memory (PROM) or read-only-memory asdetailed in U.S. Pat. No. 4,119,946. By using the Hamming errorcorrection to RFID memory, the data to be stored in RFID memory isprocessed by an algorithm where it is divided into blocks, each block istransformed to a code using a code generator matrix, and the code iswritten to the RFID memory. After the code has been read back from theRFID memory, it is processed by an algorithm that includes aparity-check matrix that can detect single-bit and double-bit errors,but only the single bit errors can be corrected.

The BCH (Bose-Chaudhuri-Hocquenghem) error correction is a polynomialcode over a finite field with a particularly chosen generatorpolynomial, see for example U.S. Pat. No. 4,502,141. The data to bestored in RFID memory is transformed to a code by using an algorithmbased on a generator polynomial, and the code is written to the RFIDmemory. After the code has been read back from the RFID memory, it isprocessed by an algorithm that includes calculating roots of apolynomial to locate and correct errors. The Reed-Solomon code can beconsidered a narrow-sense BCH code.

Referring to FIG. 3, the memory chip 201 includes a complementarymetal-oxide semiconductor (CMOS) chip 201 a with a ferroelectric randomaccess memory (FRAM) 201 b.

Memory chip 201 includes the (CMOS) chip or CMOS circuitry 201 a and theFRAM circuitry 201 b as a part of the RFID tag 102 incorporated into adisposable bioprocess component 101 and preventing its unauthorized use.The examples of the CMOS circuitry 201 a components include a rectifier,a power supply voltage control, a modulator, a demodulator, a clockgenerator, and other known components.

The memory chip 201 that includes a CMOS circuitry and a digital FRAMcircuitry is called here “FRAM memory chip”. In order to achieve abilityto use the memory chip 201 device of an RFID tag 102 for authenticationof a gamma-sterilized disposable bioprocess component 101, it iscritical to address: (1) limitations of the non-volatile memory materialsuch as ferroelectric memory material and any other non-charge-basedstorage memory MATERIAL and (2) limitations of the CMOS circuitry 201 aof the memory chip 201 as a whole DEVICE upon exposure to gammaradiation.

In general, here are examples of non-volatile memory that are applicablefor the purpose of this invention are Giant Magneto-Resistance RandomAccess Memory (GMRAM), Ferroelectric Random Access Memory (FRAM), andChalcogenide Memory (GM) as described in Strauss, K. F.; Daud, T.,Overview of radiation tolerant unlimited write cycle non-volatilememory, IEEE Aerospace Conf. Proc. 2000, 5, 399-408.

Here are examples of materials that can be used to create ferroelectricmemory include potassium nitrate (KNO₃), lead zirconate titanate(PbZr_(1-x)Ti_(x)O₃, usually abbreviated as PZT), Pb₅Ge₃O₁₁, Bi₄Ti₃O₁₂,LiNbO₃, SrBi₂Ta₂O₉, and others. In ferroelectric memory, theferroelectric effect is characterized by the remnant polarization thatoccurs after an electric field has been applied. The unique chemicalatomic ordering of ferroelectric materials allows a center atom in thecrystal lattice to change its physical location. The center atom in acubic PZT perovskite crystal lattice will move into one of the twostable states upon an external applied electric field. After theexternal electric field is removed, the atom remains polarized in eitherstate; this effect is the basis of the ferroelectric as a nonvolatilememory. An electric field can reverse the polarization state of thecenter atom, changing from a logic state “0” to “1” or vice versa. Thisnonvolatile polarization, which is the difference between the relaxedstates (the charge density) is detected by the detector circuitry. FRAMis a type of memory that uses a ferroelectric material film as adielectric of a capacitor to store RFID data. On the material level, itis well known that while FRAM is more gamma radiation resistant thanEEPROM (Electrically Erasable Programmable Read-Only Memory), it stillexperiences gamma-irradiation effects. The common gamma radiationsources are cobalt-60 (Co⁶⁰) and cesium-137 (Cs¹³⁷) isotopes. The cobalt60 isotope emits gamma rays of 1.17 and 1.33 MeV. The cesium 137 isotopeemits gamma rays of 0.6614 MeV. This energy of the gamma radiation forthe Co⁶⁰ and Cs¹³⁷ sources is high enough to potentially causedisplacement damage in the ferroelectric material. Indeed, after anexposure to a gamma radiation, FRAM experiences the decrease in retainedpolarization charge due to an alteration of the switchingcharacteristics of the ferroelectric due to changes in the internalfields. This radiation-induced degradation of the switchingcharacteristics of the ferroelectric is due to transport and trappingnear the electrodes of radiation-induced charge in the ferroelectricmaterial. Once trapped, the charge can alter the local field around thedipoles, altering the switching characteristics as a function of appliedvoltage. Two known scenarios for trap sites are at grain boundaries orin distributed defects in the ferroelectric material, depending on thefabrication method of FRAM (for example, sputtering, sol-gel deposition,spin-on deposition, metal-organic chemical vapor deposition, liquidsource misted chemical deposition). In addition to the charge trapping,gamma radiation can also directly alter the polarizability of individualdipoles or domains.

On the device level, the FRAM memory chip 201 of the RFID tag 102consists of a standard electric CMOS circuit 201 a and an array offerroelectric capacitors in which the polarization dipoles aretemporarily and permanently oriented during the memory write operationof the FRAM. On the device level, the FRAM device has two modes ofmemory degradation that include functional failure and stored dataupset. Thus, the radiation response effects in the memory chip 201 is acombination of non-volatile memory 201 b and the CMOS 201 a componentsin the memory chip 201. Radiation damage in CMOS 201 a includes but isnot limited to the threshold voltage shift, increased leakage currents,and short-circuit latchup.

In conventional CMOS/FRAM memory devices, the gamma radiation inducedloss of device performance (the ability to write and read data from thememory chip) is dominated by the unhardened commercial CMOS componentsof memory chip 201.

Hardened-by-design techniques can be used to manufacture aradiation-hardened CMOS components of semiconductor memory. The examplesof hardened-by-design CMOS components include p-channel transistors inmemory array, annular n-channel gate structures, p-type guard rings,robust/redundant logic gates protecting latches, latches immune tosingle event effects (SEE), and some others. The hardened-by-designtechniques prevent radiation-hard latches from being set by single eventtransients (SET) propagating through the logic of the device.

Referring to FIGS. 4A and 4B, shows a block diagram of the redundantinformation storage is shown. When the same or redundant information iswritten and stored in different regions as shown in FIG. 4A, while someinformation may be lost as shown in FIG. 4B after gamma radiationsterilization. After the irradiation of the memory chip 201, the methodfor redundant information storage provides a reliable storage of theinformation in at least one remaining non-damaged regions of the FRAMmemory chip 201. FRAM is a non-volatile memory 201 b offering high-speedwriting, low power consumption and long rewriting endurance. Thenonlimiting examples of memory chips 201 include FRAM chips for 13.56MHz such as of the FerVID family™ and are MB89R111 (ISO14443, 2 Kbyte),MB89R118 (ISO15693, 2 Kbyte), MB89R119 (ISO15693, 256 byte) availablefrom Fujitsu located at 1250 East Argues Avenue, Sunnyvale, Calif.94085.

A list of companies that can fabricate FRAM memory chips includesRamtron International Corporation (Colorado Springs, Colo.), Fujitsu(Japan), Celis Semiconductor (Colorado Springs, Colo.), and others. TheRFID tag 102 that contains the FRAM memory chip can also be convertedinto RFID sensor as described in U.S. patent application numbers US2007-0090926, US 2007-0090927, and US 2008-0012577, which are herebyincorporated by reference.

FIG. 5 is a flow chart of the operation of the disposable component withthe integrated RFID tag 102. At block 501, the RFID tag 102 isfabricated. RFID tag 102 is fabricated in three steps that include:fabrication of a FRAM memory chip 201 (FIG. 2), fabrication of antenna203, and attachment of memory chip 201 to antenna 203 using acceptablecommon or typical practices and manufacturing approaches for fabricationknown to those of ordinary skill in the art. At block 503, thedisposable bioprocess component 101 is fabricated by the typicalpractices known to those of ordinary skill in the art for fabricatingthe bioprocess component 101. As stated above, the bioprocess component101 may be for example, storage bags, bioreactors, transfer lines,filters, separation columns, connectors, and other components. Each ofthese and other components is fabricated using acceptable commonpractices and manufacturing approaches known to those of ordinary skillin the art.

After the RFID tag 102 and the disposable bioprocess component 101 arefabricated, then at block 505 the RFID tag 102 is integrated incombination with the disposable bioprocess component 101. RFID tag 102is integrated in combination with the disposable bioprocess component byusing the method known to those of ordinary skill in the art oflamination or molding the RFID tag 102 into the part of the disposablebioprocess component 101 or attaching the RFID tag 102 to the disposablebioprocess component 101. Also, there are other known ways to integrateRFID tags 102 into disposable bioprocess component 101.

At block 507, the redundant data is written onto the memory chip 201 ofthe RFID tag 102. The approach to writing redundant data onto the memorychip 301 is illustrated in FIG. 6, which improves the reliability ofwriting and reading data onto gamma radiation resistant RFID tags. Forthis approach, the total available memory of the memory chip 201 isdivided into three sectors: sector A for article identification (ID)information, serial number and possible sensor calibrations, sector Bfor authentication information and sector C with user available blocks.Sector A may be referred to as a first sector, sector B may be referredto as a second sector and sector C may be referred to as a third sector.Even though, there is only one memory chip 201 depicted here a pluralityof memory chips may be utilized, for example 1 to 100 memory chips,included in one or more RFID tags. Also, even though this memory chip201 only has three sectors the memory chip may have 1 to 100 or moresectors.

The redundant data is written into each sector A, B and C. Redundancy isachieved by writing multiple copies of the data into each sector A, Band C.

Referring to FIG. 8, there is a table illustrating how the redundantinformation is stored on sectors A, B and C. For example, theimprovement of reliability of writing and reading data onto RFID tagsafter their gamma irradiation was demonstrated using memory chipsMB89R118A (Fujitsu). These memory chips are made using a standard 0.35micrometers CMOS circuitry process coupled with a process ofmanufacturing ferroelectric memory. These memory chips were attached to5.5×8.5 cm antenna. Writing and reading of data was performed using acomputer-controlled multi-standard RFID Reader/Writer evaluation module(Model TRF7960 Evaluation Module, Texas Instruments) and a reader/writer111 from Wave Logic LLC (Scotts Valley, Calif.).

The total available 2000 bytes memory of memory chips was divided intothree sectors such as a sector A for article ID, serial number, andpossible sensor calibrations, sector B for authentication, and sector Cwith user available blocks. Redundant data was written into two sectors(A and B). The sectors A, B, and C were unencrypted data, encrypteddata, and empty (no data), respectively. The respective page redundancywas 11, 9, and 5, thus we had 25 pages (11+9+5=25) of 80 bytes per page.The goal was to write redundant data, gamma irradiate the tags, read thedata back, and count the number of pages that were correct after theirradiation. We developed an algorithm that compared the content of eachpage and highlighted the page that had a content that did not match withthe majority of similar pages.

It was found that one of pages A was corrupted after gamma irradiation(35 kGy) in one tag out of 13 tags. However, because the majority ofsimilar pages had identical data, the overall data was correctlyidentified. As a result of the redundant data writing onto ferroelectricmemory, each tag out of 13 tested tags was correctly read and thus, alltags passed the gamma irradiation test, although one page (80 bytes) wascorrupted by gamma radiation.

For another example, the improvement of reliability of writing andreading data onto RFID tags after their gamma irradiation wasdemonstrated using memory chips MB89R118A (Fujitsu). These memory chipsare made using a standard 0.35 micrometers CMOS circuitry coupled with aferroelectric memory. These memory chips were attached to 5.5×8.5 cmantenna. Details of writing and reading of data and the method ofredundancy of writing data was described in the first example.

Before irradiation the read range of the tested RFID tags with memorychips based on CMOS circuitry and ferroelectric memory was from 10 to 50mm from the reader. It was unexpectedly found that immediately afterirradiation with 35 kGy of gamma rays, the read range became verynarrow, 20-21 mm from the reader. The read range became 12-30 mm after 2weeks after gamma irradiation. The read range found after irradiationdid not reach the initial read range after months after the irradiation.To read reliably the RFID tags after gamma irradiation the power levelof the employed RFID reader was altered from its minimum to its maximumand the tag response was determined To read reliably the RFID tags aftergamma irradiation, the distance between the employed RFID reader and theRFID tag was altered from its minimum to its maximum distance before thetag gamma irradiation and the tag response was determined

For example 3, the release of additional memory blocks for the end-userafter the gamma irradiation was demonstrated after the redundancy ofwritten data was implemented. RFID tags 102 with ferroelectric memoryand with redundant data were used as described in Example 1. After theirradiation, the data was read from the memory of ferroelectric memorychips. The correct data was established from the at least threeidentical pages. Thus, the rest of the pages were released for the enduser.

Referring to FIG. 7, this figure shows the operation of the memory chip201. Text or data is written onto the memory chip. Redundant data iswritten in sequence into the memory of the memory chip 201 using adigital reader/writer 111 (FIG. 1) device for example from TexasInstruments, Wave Logic, etc. Typically, the reader/writer is called areader. The RFID reader 111 operates with the RFID tag 102 where theRFID tag 102 is composed of the antenna coil 203 and the memory chip 201(FIG. 3) that includes basic modulation circuitry (on-boardrectification bridge and other RF front-end devices) 201 a andnon-volatile memory 201 b. The tag 102 is energized by a time-varyingelectromagnetic radio frequency (RF) wave (called a carrier signal) thatis transmitted by the reader 111. The reader is a microcontroller-basedunit with a wound output coil, peak detector hardware, comparators, andfirmware designed to transmit energy to a tag and read information backfrom it by detecting the backscatter modulation. When the RF fieldpasses through an antenna coil, an AC voltage is generated across thecoil. This voltage is rectified by the modulation circuitry of thememory chip 201 to supply power to the tag 102. The information storedin the tag 102 is transmitted back (backscattered) to the reader 111.The reader 111 demodulates the signals received from the tag antenna203, and decodes the signal for further processing. The memory chip 201is connected to the tag antenna 203.

During the writing process, an encoding algorithm that is stored on thechip 201 is used to encode the text/data. After encoding (encryption)completion, text/data, the encoded (encrypted text/data) is read fromthe memory chip 201. It further is directed into an external decodingalgorithm that operates in combination with reading of a tag ID value.The tag ID value in combination with the external decoding algorithmproduces a decoded text/data.

Referring to FIG. 5, at block 509, the disposable component 101 with anintegrated RFID tag 102 is sterilized, such as by radiationsterilization or gamma-sterilization. The gamma sterilization process isdescribed in: Baloda, S.; Martin, J.; Carter, J.; Jenness, E.; Judd, B.;Smeltz, K.; Uettwiller, I.; Hockstad, M., Guide to Irradiation andSterilization Validation of Single-Use Bioprocess Systems, Part 1,BioProcess International 2007, September, 32-40 which are herebyincorporated by reference. Radiation sterilization is a common means ofmicrobial controland sterilization applied to single-use systems. Gammairradiation is the application electromagnetic radiation (gamma rays)emitted from radionuclides such as Cobalt 60 (60 Co) and Cesium 137 (137Cs) isotopes. Gamma rays are not retarded by most materials and canpenetrate through most single-use bioprocess system components.Microorganisms are inactivated by damage to their nucleic acidsresulting from ionizing irradiation. Gamma rays are also not retained bymaterial and leave no residual radioactivity. Gamma irradiation dosageis measured in kilogray (kGy) units, which quantify the absorbed energyof radiation. One gray is the absorption of one joule of radiationenergy by one kilogram of matter (one kGy=one joule/gram). A conversionfrom megarad to kilogray is:

-   1 megarad (Mrad)=10 kilogray, kGy.

The dosages that are greater than or equal to 8 kGy are generallyadequate to eliminate low bio;-burden levels. In cases where bioburdenlevel is elevated (>1,000 colony forming units, or cfu, per unit), asmay occur with very large single-use systems, higher doses may berequired to achieve sterility. Generally, 25 kGy can achieve sterilitywith a sterility assurance level (SAL) of 10⁻⁶. Even with elevatedbioburden levels, bioburden reduction can be achieved with lowerprobabilities of sterility (e.g., SAL of 10⁻⁵ or 10 ⁻⁴). Productsirradiated to such SALs are still sterile but have higher probabilitiesof non-sterility and may not meet standards for validated sterile claimsas specified in industry standards for sterilization of health careproducts. The gamma irradiation process uses well-defined operatingparameters to ensure accurate dosing. In a well-designed irradiationfacility, for any given density of aerial the only variable determiningthe amount of radiation the product and microorganism receives is thetime the material spends within the radiation field. Products are notexposed to heat, humidity, pressure, or vacuum. Gamma irradiationproduces minimal waste byproducts and does not require quarantine forout-gassing (as with ethylene oxide gas sterilization) or routinebiological reactivity testing. As a constant and predictablesterilization method, gamma irradiation provides benefits in safety,time, and cost.

Next, at block 511 the disposable component 101 is assembled in abiological fluid flow. Disposable bioprocess component 101, for examplemay be storage bags, bioreactors, transfer lines, filters, separationcolumns, connectors, and other components, are assembled usingacceptable common practices and manufacturing approaches known to thoseof ordinary skilled in the art.

At block 513, there is a determination if the disposable component 101(FIG. 1) is authentic. The reader 106 of the measurement device 111 isutilized to authenticate the RFID tag 102 of the disposable component101. Authentication is performed to prevent illegal use of thedisposable bioprocess components, to prevent illegal operation of thedisposable bioprocess components, and to prevent illegal pharmaceuticalmanufacturing. There is a need to authenticate products in supply chainapplications because counterfeits can be very similar or even identicalto authentic products. As described in Lehtonen, M.; Staake, T.;Michahelles, F.; Fleisch, E., From Identification to Authentication—AReview of RFID Product Authentication Techniques, In Networked RFIDSystems and Lightweight Cryptography. Raising Barriers to ProductCounterfeiting; P. H. Cole and D. C. Ranasinghe, Ed.; Springer: BerlinHeidelberg, 2008; 169-187, which are hereby incorporated by reference.RFIDs are employed for product authentication. The benefits of RFIDcompared to old authentication technologies include non line-of-sightreading, item-level identification, non-static nature of securityfeatures, and cryptographic resistance against cloning. RFID systems ingeneral comprise RFID tags, readers, and online database.

Product authentication using RFIDs can be based on RFID tagauthentication or identification and additional reasoning using onlineproduct data. Furthermore, RFID supports for secure ways to bind theRFID tag and the product. To resist cloning and forgery are the mostimportant security properties of authentication RFID tags.

There are several RFID product authentication approaches. One productauthentication approach is unique serial numbering. By definition, oneof the fundamental assumptions in identification, and thus also inauthentication, is that individual entities possess an identity. Insupply chain applications, issuing unique identities is efficientlyaccomplished with RFID. There is a unique serial numbering andconfirmation of validity of identities as the simplest RFID productauthentication technique. The simplest cloning attack against an RFIDtag 102 only requires the reader 106 reading the tag serial number andprogramming the same number into an empty tag. However, there is anessential obstacle against this kind of replication. RFID tags have aunique factory programmed chip serial number (or chip ID). To clone atag's ID would therefore also require access to the intricate process ofchip manufacturing.

Another product authentication approach is track and trace-basedplausibility check. Track and trace refers to generating and storinginherently dynamic profiles of individual goods when there is a need todocument pedigrees of the disposable bioprocess product, or as productsmove through the supply chain. The product specific records allow forheuristic plausibility checks. The plausibility check is suited forbeing performed by customers who can reason themselves whether theproduct is original or not, though it can also be automated by suitableartificial intelligence. Track and trace is a natural expansion ofunique serial numbering approaches. Furthermore, track and trace can beused in supply chains for deriving a product's history and fororganizing product recalls. In addition, biopharmaceutical industry haslegislation that demands companies to document product pedigrees.Therefore, the track and trace based product authentication can becost-efficient, as also other applications to justify the expenses.

Another product authentication approach is secure object authenticationtechnique that makes use of cryptography to allow for reliableauthentication while keeping the critical information secret in order toincrease resistance against cloning. Because authentication is needed inmany RFID applications, the protocols in this approach come fromdifferent fields of RFID security and privacy. In one scheme, it isassumed that tags cannot be trusted to store long-term secrets when leftin isolation. Thus, the tag 102 is locked without storing the accesskey, but only a hash of the key on the tag 102. The key is stored in anonline database of the computer 109 connected to the reader 106 and canbe found using the tag's 102 ID. This approach can be applied inauthentication, namely unlocking a tag would correspond authentication.

Another product authentication approach utilizes product specificfeatures. In this approach the authentication is based on writing on thetag 102 memory 201 a digital signature that combines the tag 102 IDnumber and product specific features of the item that is to beauthenticated. These product specific features of the item that is to beauthenticated can be response of the integrated RFID sensor. The sensoris fabricated as a memory chip with an analog input from a separatemicro sensor. The sensor also can be fabricated as described in U.S.patent application numbers US 2007-0090926, US 2007-0090927, US2008-0012577, which are hereby incorporated by reference. These featurescan be physical or chemical properties that identify the product andthat can be verified. The chosen feature is measured as a part of theauthentication by the reader 106 and if the feature used in the tag'ssignature does not match the measured feature, the tag-product pair isnot original. This authentication technique needs a public key stored onan online database that can be accessed by the computer 109 connected tothe measurement device 111. An offline authentication can be also usedby storing the public key on the tag 102 that can be accessed by thecomputer 109 connected to the measurement device, though this decreasesthe level of security.

Gamma resistant RFID tag 102 facilitates the authentication of thedisposable component onto which it is attached. Authentication involvesverifying the identity of a user logging onto a network by using themeasurement device 111 and the reader 106 and the disposable componentor assembled component system. Passwords, digital certificates, andsmart cards can be used to prove the identity of the user to thenetwork. Passwords and digital certificates can also be used to identifythe network to the client. The examples of employed authenticationapproaches include: Passwords (What You Know) and Digital certificates,physical tokens (What You Have, for example integrated RFID sensor withits response feature); and their combinations. The use of twoindependent mechanisms for authentication; for example, requiring asmart card and a password is less likely to allow abuse than eithercomponent alone.

One of the authentication approaches using the gamma resistant RFID tag102 on the disposable component 101 involves mutual authenticationbetween reader 106 and RFID tag 102 which is based on the principle ofthree-pass mutual authentication in accordance with ISO 9798-2, in whicha secret cryptographic key is involved. In this authentication method,the secret keys are not transmitted over the airways, but rather onlyencrypted random numbers are transmitted to the reader 106. These randomnumbers are always encrypted simultaneously. A random session key can becalculated by the measurement device 111 and the reader 106 from therandom numbers generated, in order to cryptologically secure thesubsequent data transmission.

Another authentication approach is when each RFID tag 102 has adifferent cryptological key. To achieve this, a serial number of eachRFID tag 102 is read out during its production. A unique key is furtherderived using a cryptological algorithm and a master key, and the RFIDtag 102 is thus initialized. Thus, each RFID tag 102 receives a keylinked to its own ID number and the master key.

RFID tags with unique serial numbers can be authenticated and alsoaccess lot information (e.g. date of manufacture, expiration date, assayresults, etc.) from the device manufacturer. The serial number and lotinformation is transferred to a user accessible server once the producthas been shipped. The user upon installation then reads the RFID tagthat transmits the unique serial number to a computer with a secureinternet link to the customer accessible server. A match of the serialnumber on the server with the RFID tag serial number then authenticatesthe device and permits use of the device. Once the information isaccessed on the server the information is then becomes user inaccessibleto prevent reuse of a single use device. Conversely, if there is nomatch with a serial number the device cannot be used and is locked outfrom authentication and access of lot information.

To encrypt data for its secure transmission, the text data istransformed into encrypted (cipher) text using a secret key and anencryption algorithm. Without knowing the encryption algorithm and thesecret key, it is impossible to recreate the transmission data from thecipher data. The cipher data is transformed into its original form inthe receiver using the secret key and the encryption algorithm.Encryption techniques include private key cryptography and public keycryptography that prevent illegal access to internal information in thememory on the memory chip.

If it is determined that the disposable component 101 is notauthenticated then at block 515, the disposable component 101 has afailure. If there is a failure with the disposable component 101, thenthe user is warned that the disposable component 101 does not appear tobe authenticated or genuine and should be investigated. A failure can(1) generate a visual or audible alarm, (2) send a message to thedata-base provider; (3) halt execution of the process. However, if thedisposable component 101 is authenticated and has passed at block 517then the operation is allowed. If it is allowed then the disposablecomponent 101 is genuine and the performance of the task is genuine. Byensuring that only approved disposable components 101 are used, there isa reduction in the liability that a counterfeit poor quality disposablecomponent 101 is used on the hardware and a user files an unjustifiedcomplaint or those processes which were not granted export use licenseby government authorities are prohibited.

Next, at block 519 user critical digital data at the disposablecomponent 101 is released and the process ends. The disposable component101 will also allow users to access manufacturing information about theproduct—for example lot number, manufacturing data, releasespecifications etc. This data would only be available if the card reader106 was able to verify the RFID tag 102 was authentic and genuine. Thisuser critical data will be displayed on the computer 109, which also maybe connected to a typical printer, such as HP LaserJet 1200 Seriesmanufactured by Hewlett Packard, 3000 Hanover Street, Palo Alto, Calif.94304 that prints this release data.

This invention provides a system and apparatus that is able toauthenticate and prevent illegal pharmaceutical and other manufacturingand unauthorized operation of disposable bioprocess components. Thisinvention utilizes a ferro-electric random access memory chip (FRAM)chip to store redundant information on a RFID tag attached to thedisposable bioprocess components, where the redundant information iswritten in sequence into the memory chip, so that the redundantinformation can remain in the chip when the RFID tag and disposablebioprocess component is gamma-sterilized. Also, this invention includesa method for authenticating the disposable bioprocess component thatreduces liability in that a counterfeit poor quality disposablecomponent is not used on the hardware so the user will not file anunjustified complaint.

It is intended that the foregoing detailed description of the inventionbe regarded as illustrative rather than limiting and that it beunderstood that it is the following claims, including all equivalents,which are intended to define the scope of the invention.

1. A method for preventing an unauthorized use of a disposablebioprocess component the method comprising: fabricating an RFID tag thatincludes a memory chip that contains both a CMOS circuitry and a FRAMcircuitry; fabricating a disposable bioprocess component; adapting theRFID tag for physical, chemical, or biological sensing in disposablebioprocess component forming an RFID sensor; integrating the resultingRFID sensor with the disposable bioprocess component; initializing thememory chip by applying a RF signal to the CMOS circuitry; writingerror-correctable information to an FRAM portion of the memory chipwherein the error-correctable information contains calibrationparameters of the RFID sensor; sterilizing the disposable bioprocesscomponent and the integrated RFID sensor; assembling the disposablebioprocess component in a bioprocess fluid flow; and authenticating thedisposable bioprocess component and the RFID sensor.
 2. A method forpreventing an unauthorized use of a disposable bioprocess component, themethod comprising: fabricating an RFID tag that includes a memory chipthat contains a CMOS circuitry, a FRAM circuitry, and analog input froma physical, chemical, or biological sensor; attaching at least onesensor to the memory chip to form a RFID sensor; fabricating adisposable bioprocess component; integrating the RFID sensor with thedisposable bioprocess component; initializing the memory chip byapplying a RF signal to the CMOS circuitry; writing error-correctableinformation to a plurality of regions in the FRAM circuitry wherein theerror-correctable information contains calibration parameters of theRFID sensor; sterilizing the disposable bioprocess component and theintegrated RFID sensor; assembling the disposable bioprocess componentin a biological fluid flow; and authenticating the disposable bioprocesscomponent with the RFID sensor wherein authentication involves RFIDsensor initialization and a change of its reading.
 3. The method ofclaim 2, wherein the sensor is from the group consisting of physicalsensor, chemical sensor, or biological sensor.
 4. A method forpreventing an unauthorized use of a disposable bioprocess component, themethod comprising: fabricating an RFID tag with a memory chip thatcontains both a CMOS circuitry and a FRAM circuitry; fabricating adisposable bioprocess component; integrating the RFID tag with thedisposable bioprocess component; initializing the memory chip byapplying a RF signal to the CMOS circuitry and writing redundantinformation to a plurality of regions in the FRAM circuitry;gamma-sterilizing the disposable bioprocess component with theintegrated RFID tag; assembling the disposable bioprocess component in abiological fluid flow, and authenticating the disposable bioprocesscomponent with the RFID tag when RFID tag reading is performed atdifferent power levels of the RFID tag reader or at different distancesbetween the reader and the RFID tag.